Nielander Adam C, Blair Sarah J, McEnaney Joshua M, Schwalbe Jay A, Adams Tom, Taheri Sawson, Wang Lei, Yang Sungeun, Cargnello Matteo, Jaramillo Thomas F
Department of Chemical Engineering, Stanford University, 443 Via Ortega, Stanford, California 94305, United States.
Adams & Chittenden Scientific Glass, 2741 Eighth Street, Berkeley, California 94710, United States.
ACS Omega. 2020 Jul 2;5(27):16455-16459. doi: 10.1021/acsomega.0c00742. eCollection 2020 Jul 14.
The recirculation of gases in a sealed reactor system is a broadly useful method in catalytic and electrocatalytic studies. It is especially relevant when a reactant gas reacts slowly with respect to residence time in a catalytic reaction zone and when mass transport control through the reaction zone is necessary. This need is well illustrated in the field of electrocatalytic N reduction, where the need for recirculation of N has recently become more apparent. Herein, we describe the design, fabrication, use, and specifications of a lubricant-free, readily constructed recirculating pump fabricated entirely from glass and inert polymer (poly(ether ether ketone) (PEEK), poly(tetrafluoroethylene) (PTFE)) components. Using these glass and polymer components ensures chemical compatibility between the piston pump and a wide range of chemical environments, including strongly acidic and organic electrolytes often employed in studies of electrocatalytic N reduction. The lubricant-free nature of the pump and the presence of components made exclusively of glass and PEEK/PTFE mitigate contamination concerns associated with recirculating gases saturated with corrosive or reactive vapors for extended periods. The gas recirculating glass pump achieved a flow rate of >500 mL min N against atmospheric pressure at 15 W peak power input and >100 mL min N against a differential pressure of +6 in. HO (∼15 mbar) at 10 W peak power input.
在密封反应器系统中进行气体再循环是催化和电催化研究中一种广泛有用的方法。当反应气体在催化反应区的停留时间内反应缓慢且需要通过反应区进行传质控制时，这种方法尤为重要。这一需求在电催化氮还原领域得到了很好的体现，近期对氮气再循环的需求愈发明显。在此，我们描述了一种完全由玻璃和惰性聚合物（聚醚醚酮（PEEK）、聚四氟乙烯（PTFE））部件制成的无润滑、易于构建的再循环泵的设计、制造、使用和规格。使用这些玻璃和聚合物部件可确保活塞泵与广泛的化学环境具有化学兼容性，包括电催化氮还原研究中常用的强酸性和有机电解质。泵的无润滑特性以及仅由玻璃和PEEK/PTFE制成的部件减少了与长时间再循环充满腐蚀性或反应性蒸汽的气体相关的污染问题。该气体再循环玻璃泵在峰值功率输入为15 W时，相对于大气压力实现了>500 mL min N的流速，在峰值功率输入为10 W时，相对于+6 in. HO（约15 mbar）的压差实现了>100 mL min N的流速。
